This project describes the intramural formulation activities with potential antineoplastic agents. Several of the agents investigated were poorly water soluble symmetrical compounds that contained at least two identical labile groups NSC-182986, aziridinyl benzoquinone; NSC-172112, spirohydantoin mustard; and diacetylmorphine hydrochloride. High performance liquid chromatographic methods were developed for NSC-182986 and diacetylmorphine using reverse phase columns. Hydrolysis was studied over a wide pH range and degradation products were characterized. Additional studies involved a sensitive method for the estimation of amygdalin in human urine. A degradative method was developed that involved hydrolysis by beta-glucosidase plus alkali to yield glucose, cyanide and benzaldehyde. The latter was extracted into methylene chloride and measured by ultraviolet absorbance.